反应详情

温度

110 °C

To a suspension of [(2-chlorophenyl)amino]-N-[5-(bromomethyl)-2-methylthiopyrimidin-4-yl]carboxamide (1360 g, 3.62 mole) of in 10 L 1-methyl-2-pyrrolidinone was added 136 mL hexamethyldisilazane. The mixture was heated to an internal temperature of 105-115° C. for 1.5 hours. The mixture was then cooled to 30° C. and treated with 20L water. The mixture was then stirred at 5-8° C. for 2 hours and filtered. The filters were collected and washed sequentially with water and hexanes. The product was placed in a drying oven and heated under vacuum for 16 hours to give 780 g (70.1%) of 3-(2-chlorophenyl)-7-methylthio-3,4-dihydropyrimido[4,5-d] pyrimidin-2(1H)-one (sulfide 10.1) as an off-white solid. (M+1 308)

1. temperatureThe mixture was then cooled to 30° C.
2. filtrationfiltered
3. customThe filters were collected
4. washwashed sequentially with water and hexanes
5. customThe product was placed in a drying oven
6. temperatureheated under vacuum for 16 hours